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IS 3025-54 (2003): Methods of Sampling and Test (Physical

and Chemical) for Water and Wastewater, Part 54: Nickel
[CHD 32: Environmental Protection and Waste Management]

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IS 3025 (Part 54): 2003

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Indian Standard
METHODS OF SAMPLING AND TEST (PHYSICAL AND
CHEMICAL) FOR WATERAND WASTEWATER
PART 54 NICKEL

(First Revision )

ICS 13.060.50

Q BIS 2003

BUREAU
MANAK

Februaty

2003

OF
BHAVAN,

INDIAN

STANDARDS

9 BAHADUR
SHAH
NEW DELHI 110002

ZAFAR

MARG

Price Group 3

Environment

Protection

and Waste Management

Sectional Committee,

CHD 32

FOREWORD
This Indian Standard (Part 54) (First Revision) was adopted by the Bureau of Indian Standards, after the draft
finalized by the Environment Protection and Waste Management Sectional Committee had been approved by
the Chemical Division Council.
Pol Iution caused by substances, on which biotic and abiotic agencies of decomposition
are ineffective, is a
unique type of pollution. Toxic trace elements and heavy metals come under the category of non-degradable
pol Iutants. The problem caused by these elements is in fact due to their concentration in the environment in the
bio-available state and above a certain concentration become harmful to the living organism.
Nickel is not so widely distributed in the earths crust and the nickel content in the soil is of the order of 100 pg/g.
The levels of nickel in sea water is much lower. Nickel is found in almost all human tissues, but essentially of
nickel to human being is yet to be proved. Constant exposure with nickel at higher concentrations in aqueous
solutions (from their use in the electroplating baths and in the preparation of Ni-catalysts) can lead to allergic
sensitization of the skin and what is known as Ni dermatitis. Airborne Ni and nickel compounds (both in the
soluble and in the insoluble forms even at the levels of 1mg/m3 and 10 mg/m3 respectively), are highly hazardous
and carcinogenic.
Nickel (N i) is a known carcinogen of respiratory tract. Important sources of Ni are its sulphide and oxide ores.
It is the combustion of fossil fuels which contributes the largest amount of Ni to the environment. About
70000 tons of Ni are discharged into the environment from combustion of fossil fuels alone on global scale.
About 0.03-0.12 mg of Ni is present per cubic metres of air of our crowded cities. Estimated daily intake of Ni
in human diet averages around 165 mg per day. During the past few years evidence has accumulated that Ni is
nutritionally an essential element. It is associated with the synthesis of Vitamin B 12.
People occupationally involved with refining and use of Ni are pre-disposed to nasal cancers. Nickel carbonyl
was found to be the principal carcinogen. However, it was later concluded from epidermilogical
as well as
experimental studies that Nickel sulphide could also be responsible for the carcinogen action. Most common
toxic effects produced as a sequel to Ni exposure in large amounts include dermatitis and respiratory disorders.
Ni inhibits the activity of a number of enzymes such as maleic dehydrogenase, cytochrome oxidase and isocitrate
dchydrogenase while its powder or dust is carcinogenic. Nickel carbonyl, formed as a consequence of reaction
of Ni with CO is a volatile compound which is the most toxic of all the forms of Ni. It is a carcinogen and half
an hour exposure to about 30 ppm could be lethal to human beings. The illness begins with headache, nausea,
vommiting and epigastric or chest pain which are accompanied by fever and leucocytosis. More severe cases
proceed to pneumonia, respiratory failure and eventually cerebral oedema and death.
The technical committee responsible for the formulation of IS 3025: 1964 had decided to revise the standard
and pub]ish it as separate parts. This standard is one of the different parts under the IS 3025 series of standards.
In the preparation of this standard, considerable assistance is derived from Standard Methods for the Examination
of Water and Waste Water, 19th Edition-1995, published by the American Public Health Association, Washington,
U. S. A., and Vogels Text Book of Quantitative Inorganic Analysis, 4th Edition, 1978.
Atomic absorption method as specified in this standard is technically equivalent to Method A of 1S0 8288 : 1986
Water quality Determination of cobalt, nickel, copper, zinc, cadmium and lead Flame atomic absorption
spectrometric method.
The composition

of the Committee

responsible

for formulation

of this standard is given at Annex A.

In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 Rules for rounding off numerical
values (revised).

IS 3025 (Part 54): 2003

Indian Standard
METHODS OF SAMPLING AND TEST (PHYSICAL AND
CHEMICAL) FOR WATER AND WASTEWATER
PART 54 NICKEL

(First Revision )
1 SCOPE

5 PURITY OF THE REAGENTS

1.1 This standard prescribes

determination of nickel:

two methods

a)

Dimethylglyoxime

method, and

b)

Atomic absorption

method.

for the

Unless specified otherwise, only pure chemicals

nickel free distilled water shall be used in tests.

NOTE Pure chemicals shall mean chemicals that do not

contain impurities which affect the result ofamdysis.

6 DIMETHYLGLYOXIME

1.2 Depending upon the concentration

range and
interference levels, choice of the method is made.

Nickel ions react in presence of oxidizing agents (such

as bromine), with dimethylglyoxime
to give a soluble
red coloured
complex
containing
Ni in higher
oxidation states of (III) and (IV). This complex absorbs
at 445 nm. This method is applicable in the range of
30 to 500 pg/1 of nickel.

The standards listed below contain provisions which

through reference in this text, constitute provisions of
this standard. At the time of publication, the editions
indicated were valid. All standards are subject to
revision and parties to agreements
based on this
standard are encouraged to investigate the possibility
of applying the most recent editions of the standards.

7022 (Part 1) :
1973
7022 (Rut 2) :
!979

METHOD

6.1 Principle

2 REFERENCES

IS No.
3025 (Part 1) :
1987

and

6.2 Interference
Cobalt and copper interfere in estimation of nickel.
Interference of Cu (II), Co (II) and other metals is
removed by separation of nickel. [Extraction of Ni (11)
dimethylglyoxime
in CHC13, and washing the CHCl~
layer with dilute NHAOH, and re-transferring
the
Ni (II) to aqueous phase.]

Title
Methods
of sampling
and test
(physical and chemical) for water
and wastewater : Part 1 Sampling
(jrst revision)
Glossary of terms relating to water,
sewage and industrial effluents, Part 1
Glossary of terms relating to water,
sewage and industrial effluents, Part 2

6.3 Apparatus
6.3.1 Spectrophotometer

3 TERMINOLOGY

6.3.2 Standard

For the purpose of this standard, definitions given in

IS 7022 (Part 1) and IS 7022 (Part 2) shall apply.

6.3.3 pH Meter

for use at 445 nm.

Volumetric Glasswares

6.4 Reagents
6.4.1 Ammonium
and 0.5 N.

4 SA.MPLING AND STORAGE

The sampling shall be done as prescribed in IS 3025
(Part 1). The sampling
bottles shall be cleaned
thoroughly with dilute nitric acid (6N), prior to the
final rinsing with water. The water samples should be
collected and stored preferably in pol ypropylene bottles
or chemically resistant glass containers. The analysis
of such samples is to be carried out within 24 h of
sampling. For the preservation, the samples should
be acidified with concentrated nitric acid (2 ml ofconc
nitric acid in 1 litre sample, just to bring down the pH
below 2). The acidified samples can be stored for a
few days (up to 5 days) in a refrigerator.

6.4.2 Hydrochloric
0.5 N.

Hydroxide

concentrated

Acid concentrated

(14 N)

(11 N) and

6.4.3 Citric Acid 10 percent WIVin water.

6.4.4 Dimethylglyoxime
alcohol.

1 percent

WIV in ethyl

6.4.5 Ethyl Alcohol 95 percent (v/v).

6.4.6 Chloroform
6.4.7 Bromine Water Saturated water with bromine.

IS 3025 (Part 54) :2003

6.4.8 Standard Nickel Solution

funnel and extract the Ni-dimethylglyoxime

complex
with three 5 ml portions of chloroform.
Shake the
combined chloroform extract with 10 ml of 0.5 N
ammonia sofution. Separate the two layers. Collect
the ammonia washings into another separator
funnel
and shake the ammonia washings
with 2 ml of
chloroform. Transfer this chloroform layer to the main
chloroform layer, and discard the aqueous-ammonia
phase. Nickel present in the chloroform
phase is
returned back to an aqueous phase, by shaking the
chloroform layer with two 5 ml portions of 0.5N HCI.
Transfer quantitatively the hydrochloric acid layer into
a 100 ml volumetric flask. Add about 10 ml of water,
2 ml of saturated bromine water and 2 ml of cone
ammonia solution to it. Cool to room temperature,
add 1 ml of dimethylglyoxime
solution and dilute to
100 ml with water. Measure the absorbance of the
nickel complex at 445 nm after 5 min against the
reagent blank (prepared in an identical manner using
water in place of the sample solution).

Dissolve 0.673 g of ammonium

nickel sulphate
[NiSOq(NHd)2 SOd.6H20], in a small quantity of water,
and transfer quantitatively into a 1 000 ml volumetric
flask. Dilute upto the mark with water (1.0 ml = 100 pg
of Ni).
6.5 Procedure
6.5.1 Calibration

Curve

Pipette out appropriate portions of standard nickel

solution into 100 ml volumetric flasks to contain from
50 to 250 pg of Ni. For the reagent blank pipette out
10 ml of water into a separate 100 ml volumetric flask.
To each flask, add 5 ml of O.5N HC1, 2 ml of bromine
water, and 2 ml of cone ammonium hydroxide. Cool
to room temperature, add 1 ml of dimethylglyoxime
reagent and dilute up to the mark with water. Measure
the absorbance at 445 nm after 5 min. Use a reagent
blank prepared in an identical manner, using 10 ml
of water. Construct a calibration curve by plotting
absorbance values against micrograms of nickel in 100
ml of the final solution.
6.5.2 Digestion

6.6 Calculation
mg Ni/1 = Kg of Ni (in 100 ml of the final solution) ~ ~oO
yxv*

with HJO~-HN03

Transfer a suitable volume of homogenized sample to

a beaker. (Sample volume depends upon the expected
Ni content. If the expected Ni concentration is of the
order of 1 mg/1, the sample volume will be about
800 ml. If it is between 10 to 100 mg/1, about 100 ml
of the sample will be sufficient.) For preparation of
the reagent blank measure equal volume of water in a
separate beaker. Add 5 ml of cone HNO~ and a few
porcelain pieces or glass beads. Heat to boil the
solutions, and concentrate carefully on a hot plate to
lowest possible volume, cool the solution and transfer
quantitatively, to a beaker of smaller size (say 150 ml
beaker). Add 5 ml of cone HNOJ and 10 ml of cone
H~SOA. Heat up to the evolution of dense white fumes
of SOj. If the solution are not clear add 5 ml of HNO~
and reheat until a clear solution (no evolution of brown
fumes) results. Cool and transfer quantitatively into a
100 ml volumetric flask. Dilute upto the mark with
water, and mix well. Use this solution
for the
determination of nickel as described in 6.5.3.
6.5.3 Determination

where
VI = volume in ml of the sample taken for the
acid digestion, and
v,

= volume in ml of the digestion solution

taken for the final Ni determination.

7 ATOMIC

ABSORPTION

METHOD

(DIRECT)

7.1 Principle
The nickel content of the sample is determined by
atomic absorption spectrophotometry.
For dissolved
nickel the filtered sample may be directly aspirated to
the atomizer. For total recoverable
nickel, HNOJH2S00 digestion is to be carried out prior to aspiration
of the sample. This method is applicable in the range
from 0.3 to 10 mg/1. However, the concentration range
will vary with the sensitivity of the instrument used.
7.2 Interferences
The presence of high concentration
of iron and
chromium
may increase the nickel signal. Most
interference may be eliminated by the use of the nitrous
oxide acetylene flame but nickel sensitivity will be
lowered.

of Nickel

Pipette out a portion of the acid digestion solution

(containing from 50 to 250 ~g Ni) into a beaker. Add
5 ml citric acid solution.
Neutralize
with cone
ammonia solution and add a few drops in excess
@H >7.5 ensure with a pH meter or the pH paper of
appropriatepH range). Add 2 ml ofdimethylglyoxime
solution (ifCu or Co is present, more of reagent, about
5 ml is added). Transfer quantitatively into a separato~

7.3 Apparatus
7.3.1 Atomic absorption spectrophotometer
with airacetylene flames. Hollow-cathode lamp or electrodeless
discharge lamp for use at 232.0 nm.
2

IS 3025 (Part 54) :2003

7.4 Reagents
7.4.1 Hydrochloric Acid concentrated
and 10 percent V,iv.
7.4.2 Nitric Acid concentrated
(1 : 499),

(16 N) and dilute

7.4.3 Sulphuric Acid concentrated

7.4.4

( 11 N), 1:1

(36 N).

Stock Nickel Solution

Dissolve 1.273 g of nickel oxide in a minimum

quantity
of 10 percent (v/v) HC1 and transfer
quantitatively into a 1 000 volumetric flask. Dilute
upto the mark with water (1 ml = 1.0 mg of Ni).
7.4.5 Standard

Nickel Solution

Pipette out 10.0 ml of stock nickel solution into a

1000 ml volumetric flask and make upto mark with
water ( 1.0 ml = 10 pg of Ni).

time of sampling, is required. For total recoverable

nickel, HNOj-H2SOq digestion is to be carried out
(see 6.5.2).
7.5.4 Add 0.5 ml of nitric acid to a suitable volume
of the sample taken (or the solution obtained after
digestion which contains 50 to 60 yg of nickel) in a
100 ml volumetric flask. Makeup to the mark. Rinse
the nebulizer by aspirating water containing 1.5 ml
of cone HNO# Aspirate the reagent blank and carry
out zero adjustment. Aspirate the sample solution
and measure the absorbance at 232.0 nm. Determine
micrograms
of nickel in the solution
from the
absorbance reading, by referring to the calibration
curve.
7.6 Calculations
7.6.1 Soluble Nickel (direct determination
digestion step)

7.5 Procedure
7.5.1 Calibration

Curve

Prepare standard solutions containing O to 60 pg/1 of

nickel by diluting suitable volumes of standard nickel
solution with nitric acid (1 : 499) to 100 ml in
volumetric
flasks. Prepare a reagent blank in an
identical manner using 10 ml of water. Aspirate the
reagent blank and carry out zero adjustment. Aspirate
sequentially the standard solutions and measure the
absorbance at 232.0 nrn.
7.5.2 Construct
a calibration
curve by plotting
absorbance values against micrograms of Ni in 100 ml
of the final volume. Ensure that the calibration curve
is linear by making the necessary changes in the
volume of the standard solution used.
7.5.3 Determination

of Nickel

For the determination

of dissolved nickel content,
filtration through 0.45 ~m membrane filter, at the

mgNi/1 =

without the

pg of Ni (in 100 ml of the final solution) ~ ~00

v

where
V

= volume in ml, of the sample used.

7.6.2 Total Nickel (when digestion

is carried out)

pg of Ni (in 100 ml of the final solution) ~ 100

mgNi/1 =

~xv2

where

v, = volume in ml of the sample used, and

v, = total volume in ml of digested solution
used for Ni estimation.
7.6.3 Precision

and Accuracy

The relative standard

deviation
reported
literature for the Ni at 4.0 mg/1 concentration
9.8 percent.

in the
level is

IS 3025 (Part 54) :2003

ANNEX A
(Foreword)
COMMITTEE
Environment

Protection

and Waste

COMPOSITION
Management

Sectional Committee,

CHD 32

Representative(s)

Orgcmi:ation
(cntml Pollution Control Board. Delhi

SHRIDILIP BISWAS(Chairman)

A utumot i~c Research Association of [ndia, Pune

RepreSentatiVe

Bhabha Atomic Rescwch Centre, Mutmbai

DR S. SADASHIVAN

Bhwat Hetivy Electrical

DRN. G. SHRJVASTAVA

DR T. N. MAHADEVEN
(Alternate)
Limited, Haridwar

Ccnwnt Manufacturers Association, New Delhi

DR K. C. NARANG

CcaWJl Fuel Research Institute. Dhanbad

DR GULAESINGH

(cntral Leather Research Institute, Chennai

DR S. RAJAMANI

(cntml Nlechanical Engineering Research Institute, Durgap~]r

REPRESENAmVE

Ccmral Mining Research Institute, Dhanbad

DR B. K. TEWAItY

Ccntml Pollution Control Board, New Delhi

DR S. D. MAKHIJANI

Confederation of [ndian Industries (CM), New Delhi

SHIU A. K. GHOSE

Department of Industrial Policy& Promotion, New Delhi

REPRFSETWATJVE

Department of Science& TecbnoIogy (TIFAC), New Delhi

REPREXNTATIVE

Dircctcmite General Factory Advice Service and Labour Institute,

Mumbai

SHRIS. S. GAOTAM

Dmxlorate General of Health Services, New Delhi

DR (SHRJMAm)MADHURISHARMA

Engineers India Limited, New Delhi

SHRIB. B. LAL

i3virotecb Instruments Private Limited, New Delhi

SHRIRAKESHAGARWAL

Food Research & Analysis Centre, New Delhi

DR S. K. SAXENA

(;uj:lmt iollution Control Board, Ahmedabad

KUMARIP. S. SHAH

}lmdustan Lever Limited, Mumbai

SHRIB. B. DAVE

lndIaII Chemical Manufacturers Association, Mumbai

SHRIV. N. DAS
SHRIA. A. PANJWANI(Alternate)

Indian Council of Agricultural Research, New Delhi

WPRE5ENTATIW

Indian Council of Medical Research, New Delhi

SHRIH. N. SAIYAO

lmhan Inmtutc of Packaging, Mumbai

SHRIS. C. ADAK

I[CL, Vadodara

SHRIP. VUAYRAGWAVAN

DR L. C. RANE (Alternate)

DR C. S. SHARMA(Alternate)

SHRIR. P. SHARMA
(Alternate)

SHar M. R. ~JPUT (A/ternale)

SHRIRAJENDRAPRASAO(Alternate)
DR R. PRABHARARAN
(Alternate)

SHRIADITVAJHAVAR(Alfernafe)

DR J. D. DESAI (Alternate I)

SHRJH.

K. DUBEY (Alternate II)

IIdustriai Toxicology Research Centre, Lucknow

REPRESENTATIVE

hlinistry of Defcncce (R&D), DRDO, New Delhi

REPR2sE~ATtvE

Ministry of Environment and Forests, New Delhi

REPRESENTATIVE

klinistry ot_NowConventional

SHRIANIL KUMARVARSHNEY

Energy Research, New Delhi

hlinistry of Urban Development, New Delhi

REPREsWATtvE

Mun]c)pal Corpomtimr of Delhi, New Delhi

REPRESENrATrVS

Municipal Corporation of Greater Mumbai, Mumbai

REPRESENTATIVE

National Institute of Occupational Health (lCMR), Ahmedabad

DR D. J. PARIKH
DR T. S. PATEL(Aiternufe)

(Continaed

on page 5)

IS 3025 (Part 54) :2003

( ( ojirillued from page 4)

Representative(s)

Organization

DR V. I. PANDIT

National Environmental Engineering Research Institute, Nagpur

DR TAPASNANDY (Alternate I)
DR A. V. SHEKDAR(Alternate 11)

National Organic Chemical Industries Limited, Mumbai

SHRIB. K. CHOPRA

National Productivity Council, New Delhi

SHRI R. C. MONGA

N:ltiollal Themlal Power Corporation Limited, New Delhi

REPRESENTATIVE

WCBM,

REPRESENTATWE

SHIUB.

V. BAPAT(Alternate)

DR A. K. SAXENA(Alternate)

New Delhi

Pestlcldcs Association of India, New Delhi

SHRIP. N. PARME.SHAWARAN

Shriraln Iaslitute of Industrial Research, New Delhi

REPRESENTATWE

S(; S India Limited. Chennai

SHRiS. RAVI

Standardization Testing and Quality Certification Directorate. New Delhi

REPRESEi-WATWE

Steel Authority of India Limited, New Delhi

DR MEENAKSHIKAKKAR
SHRJJ. KUMAR(Alternate I)
DR V. M. SHAHSTRI(Ahernate II)

The Fertilizer Association of India, New Delhi

DR (SHIUMATI)B. SWAMiNATHAN

Thermax Limited, Pune

RE.Fw&iW4mvE

BIS D:rec:orate General

SHRIS. K. CHAUDHURLDirector & Head (CHD)

DR S. NAND (Alternate)

[Representing Director General (E@jicio)]

Member Secretary
SHRIN. K.. PAL

Director (CHD), BIS

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under the Bureau
harmonious
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in writing of BIS. This does not preclude the free use, in the course of
implementing
the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.
Review of Indian Standards
Amendments are issued to standards as the need arises on the basis
periodically; a standard along with amendments is reaffirmed when
needed; if the review indicates that changes are needed, it is taken
should ascertain that they are in possession of the latest amendments
B] S Catalogue and Standards: Monthly Additions.
This Indian Standard has been developed

from Doc : No. CHD 32 (1013).

Amendments
Amend No.

of comments. Standards are also reviewed

such review indicates that no changes are
up for revision. Users of Indian Standards
or edition by referring to the latest issue of

Issued Since Publication

Date of Issue

Text Affected

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